CN102008951A - Mo-C-codoped method for preparing one-dimensional titanate nanobelt photocatalyst material - Google Patents

Mo-C-codoped method for preparing one-dimensional titanate nanobelt photocatalyst material Download PDF

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CN102008951A
CN102008951A CN 201010538760 CN201010538760A CN102008951A CN 102008951 A CN102008951 A CN 102008951A CN 201010538760 CN201010538760 CN 201010538760 CN 201010538760 A CN201010538760 A CN 201010538760A CN 102008951 A CN102008951 A CN 102008951A
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photocatalyst material
metatitanic acid
tio
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CN102008951B (en
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刘曰利
陈文�
舒威
蔡祎
周静
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Wuhan University of Technology WUT
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Abstract

The invention relates to a method for preparing a one-dimensional titanate nanobelt photocatalyst material. A Mo-C-codoped method for preparing the one-dimensional titanate nanobelt photocatalyst material is characterized by comprising the following steps of: (1) dissolving butyl titanate in absolute ethanol and adding the glacial acetic acid according to a ratio of the butyl titanate to the absolute ethanol to glacial acetic acid of 45mL:180mL:4.5mL, regulating the pH value to be 3.0 by using concentrated nitric acid, and stirring; (2) adding aqueous solution of ammonium molybdate according to a mass ratio of Mo element to Ti element of 0.1 to 6 percent so as to prepare Mo-doped TiO2 powder; (3) dissolving the Mo-doped TiO2 powder and glucose in solution of sodium hydroxide according to a ratio of the Mo-doped TiO2 powder to the glucose to the solution of sodium hydroxide of 3.33g:0.1-1.5g:100mL so as to prepare turbid liquid; (4) regulating the pH value to be 7.0 by dipping HCl solution by adopting a hydrothermal method; and (5) filtering and drying to prepare the one-dimensional titanate nanobelt photocatalyst material. The method is simple in technology and high in repeatability, meets the environmental requirement and has obvious photocatalytic enhancement effect.

Description

The Mo+C codope preparation method of one dimension metatitanic acid nanometer band photocatalyst material
Technical field
The present invention relates to one dimension metatitanic acid (H 2Ti 5O 113H 2O) preparation method of nanometer carrying material belongs to nano material and field of nanometer technology.
Background technology
The development of society has brought the aggravation of polluting, and waste water from dyestuff is one of focus of present world people care, and the association area of semiconductor catalytic oxidation has caused extensive studies.TiO 2Sill has avirulence, and stability can reuse, characteristics such as photocatalytic effect height, and simultaneously to the free of contamination utilization of solar energy, being allowed to condition at has very big application prospect in the wastewater treatment, but present TiO 2Owing to self energy gap broad (3.2eV), extremely faint to the response of visible light.Therefore how improving visible light also is the key subjects of being badly in need of solution at present in the utilization of spectral region.The one dimension titanic acid nano material has special structure, as the existence in big specific area, oxygen room, interlayer structure etc., can improve and absorbs and degraded, thereby improve degradation rate.Compare TiO 2The application of material aspect photocatalysis, the research of one dimension titanate nano material is at present also less.
Though metal-dopedly can prolong TiO to a certain extent 2The photoresponse scope, but metal-doped back TiO 2Heat endurance reduce, and the metal that mixes becomes the complex centre easily, thereby reduces the activity under its ultraviolet light.In recent years, nonmetal doping can make TiO after substituting a spot of Lattice Oxygen 2Has tangible visible light activity not reducing under the photoactive situation of its ultraviolet.This brand-new discovery has caused the great interest of people, thereby makes nonmetal doping TiO 2Become a focus of photocatalysis field research.
At present, generally believe and utilize the assorted concerted catalysis effect that produces of cation-anion co-doping, can effectively remedy the shortcoming that single ionic mixes, especially can further enlarge TiO 2The light abstraction width of photochemical catalyst also improves its catalytic activity.Employing sol-gel methods such as Wang Jianbo have prepared Fe 3+-Ce 3+And La 3+-Ce 3+Codope TiO 2Photochemical catalyst, result of study show that the photocatalytic activity of codope catalyst all is higher than single doped catalyst, and this explanation codope system has better coordinative role and photocatalytic activity.Employing sol-gel methods such as Yu Shuxian have been synthesized Zn 2+, La 3+Codope TiO 2Photochemical catalyst has also carried out Optical Electro-Chemistry research, and experiment finds that codope can change the absorptivity of sample and suppress the compound of photo-generated carrier.But, do not see the one dimension H of Mo+C codope as yet because the research of codope report is less at present 2Ti 5O 113H 2The research report of the Experiment Preparation aspect of O nanometer carrying material.
Summary of the invention
The object of the present invention is to provide a kind of Mo+C codope preparation method of one dimension metatitanic acid nanometer band photocatalyst material, preparation technology is simple for this method, and is low for equipment requirements, with low cost, favorable reproducibility.
For achieving the above object, the technical solution used in the present invention is: the Mo+C codope preparation method of one dimension metatitanic acid nanometer band photocatalyst material is characterized in that it comprises the steps:
(1) press butyl titanate: absolute ethyl alcohol: glacial acetic acid=45mL: 180mL: 4.5mL, butyl titanate is dissolved in the absolute ethyl alcohol, add glacial acetic acid then, regulate pH to 3.0 with red fuming nitric acid (RFNA), stir;
(2) mass ratio by Mo element/Ti element is 0.1～6% adding ammonium molybdate aqueous solution, stirs 1h, and ultrasonic then dispersion 1.5h 80 ℃ of oven dry down, calcines 3h with the product that obtains down at 500 ℃, obtains mixing the TiO of Mo 2Powder;
(3) by the TiO that mixes Mo 2Powder: glucose: sodium hydroxide solution=3.33g: (0.1～1.5) g: 100mL, wherein the concentration of sodium hydroxide solution is 2～20M, chooses the TiO that mixes Mo 2Powder, glucose and sodium hydroxide solution; To mix the TiO of Mo 2Powder and glucose dissolve in the sodium hydroxide solution, stir 30～50h, obtain suspension solution;
(4) then, suspension solution adopts hydrothermal method hydro-thermal reaction 2～4 days under 160～220 ℃ temperature, adjusts pH value to 7.0 by dripping HCl solution;
(5) filter the back and dry 24h down, obtain one dimension metatitanic acid nanometer band photocatalyst material at 80 ℃.
The concentration of described HCl solution is 0.1M.
The invention has the beneficial effects as follows: the present invention directly adopts commercial TiO 2Powder reacts under the thermokalite hydrothermal condition as raw material, and technology is simple, and is low for equipment requirements, favorable reproducibility, and the controllable degree height meets environmental requirement, and greatly reduces synthetic cost; Has significant photocatalysis enhancement effect.
Description of drawings
Fig. 1 is the XRD figure spectrum of one dimension metatitanic acid nanometer carrying material of the different Mo+C codope content of the embodiment of the invention 1.
Fig. 2 is the appearance structure phenogram of one dimension metatitanic acid nanometer band of the 0.33%Mo+C codope of the embodiment of the invention 1.
Fig. 3 is the appearance structure phenogram of one dimension metatitanic acid nanometer band of the 0.64%Mo+C codope of the embodiment of the invention 1.
Fig. 4 is the appearance structure phenogram of one dimension metatitanic acid nanometer band of the 1.29%Mo+C codope of the embodiment of the invention 1.
Fig. 5 is the photocatalysis curve map of one dimension metatitanic acid nanometer carrying material of the different content Mo doping content of the embodiment of the invention 1.
Fig. 6 is the photocatalysis curve map of one dimension metatitanic acid nanometer carrying material of the different content Mo+C doping content of the embodiment of the invention 1.
Fig. 7 be the embodiment of the invention 1 One-Dimensional Pure metatitanic acid nanometer band, mix C metatitanic acid nanometer band, mix the change curve of benzene content behind the photocatalytic degradation benzene of 0.33%Mo metatitanic acid nanometer band and 0.33%Mo+C codope metatitanic acid nanometer carrying material.
Fig. 8 be the embodiment of the invention 1 One-Dimensional Pure metatitanic acid nanometer band, mix C metatitanic acid nanometer band, mix corresponding CO behind the photocatalytic degradation benzene of 0.33%Mo metatitanic acid nanometer band and 0.33%Mo+C codope metatitanic acid nanometer carrying material 2Content increases curve map.
The specific embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1:
The Mo+C codope preparation method of one dimension metatitanic acid nanometer band photocatalyst material, it comprises the steps:
(1) the 45mL butyl titanate is dissolved in the absolute ethyl alcohol of 180mL, adds the glacial acetic acid of 4.5mL then, regulate pH to 3.0, be accompanied by vigorous stirring with red fuming nitric acid (RFNA) (commercially available);
(2) mass ratio (0.125%, 0.25%, 0.33%, 0.64%, 1%, 1.29%, 5.15%) by different Mo element/Ti elements adds ammonium molybdate aqueous solution (being divided into 7 groups), stir 1h, ultrasonic then dispersion 1.5h, 80 ℃ of oven dry down, the product that obtains is calcined 3h down at 500 ℃, obtain mixing the TiO of Mo 2Powder;
(3) will mix the TiO of Mo 2It is that 100mL, concentration are vigorous stirring 40h in the sodium hydroxide solution of 10M that powder 3.33g and 0.20g glucose dissolve in volume, obtains suspension solution;
(4) adopt hydrothermal method hydro-thermal reaction 48h under 180 ℃ temperature then, adjust pH value to 7.0 by dripping HCl solution (0.1M);
(5) mistake is dried 24h down at 80 ℃ after filtering out filtrate, can obtain the one dimension metatitanic acid (H of Mo+C codope 2Ti 5O 113H 2O) nanometer band photocatalyst material.
The XRD figure spectrum and the SEM image of one dimension metatitanic acid nanometer band photocatalyst material are seen Fig. 1, Fig. 2-4 respectively.
Fig. 1 characterizes mutually for the thing of the one dimension metatitanic acid nanometer carrying material of different Mo+C codope content among the embodiment 1.Fig. 1 explanation: the position of each diffraction maximum of XRD figure of the synthetic product of different Mo+C codope content correspondence and relative intensity all with metatitanic acid (H 2Ti 5O 113H 2O) XRD figure of material spectrum matches (JCPDS No.:44-0131), and the thing of metatitanic acid did not change mutually after this explanation was mixed, and the doping of Mo and C is to thing not influence mutually.
Fig. 2-4: the appearance structure of the one dimension metatitanic acid nanometer carrying material of different Mo among the embodiment+C codope content characterizes.Fig. 2-4 explanation: the synthetic product of different Mo+C codope content correspondence is width about 200 nanometers, and length has several microns nanometer band.Have some less clusters simultaneously, size is between several microns are to tens microns.The different content of this explanation Mo+C does not influence the pattern of formation product-metatitanic acid nanometer band.
Fig. 5-6: the photocatalytic effect of the one dimension metatitanic acid nanometer carrying material of the Mo of different content doping and Mo+C codope among the embodiment.The slippage of benzene and the CO of correspondence behind the one dimension metatitanic acid nanometer band degraded benzene that Fig. 5-6 explanation: Fig. 5 mixes for different content Mo 2The increment of content, as can be seen from Figure 5: when the Mo/Ti ratio was 0.33% left and right sides, its catalytic efficiency reached optimum value, this moment after the illumination of 80min ultraviolet-visible benzene degraded fully, and the CO that obtains of degraded benzene 2Content is about 1000ppm.The slippage and the corresponding CO of benzene behind the one dimension metatitanic acid nanometer band degraded benzene that Fig. 6 mixes for different content Mo+C 2The increment of content, as can be seen from Figure 6: when the Mo/Ti ratio was 0.33% left and right sides, its catalytic efficiency reached optimum value, this moment after the illumination of 60min ultraviolet-visible benzene degraded fully, and the CO that obtains of degraded benzene 2Content is about 1200ppm.As seen, the Mo/Ti ratio is 0.33% o'clock, and the photocatalytic activity of corresponding Mo-C codope one dimension metatitanic acid nanometer carrying material is the highest.
Fig. 7-8: One-Dimensional Pure metatitanic acid nanometer band among the embodiment, mix C metatitanic acid nanometer band, mix the photocatalytic effect of 0.33%Mo metatitanic acid nanometer band and 0.33%Mo+C codope metatitanic acid nanometer carrying material.
Fig. 7-8 explanation: Fig. 7-8 is 0.33% o'clock for the Mo doping content, the change curve and the corresponding CO of benzene content behind the one dimension metatitanic acid nano wire degraded benzene of various doping situations 2Content increases curve, can find out very clearly from Fig. 7-8: the one dimension metatitanic acid nanometer band that C mixes is after the illumination of 80min ultraviolet-visible, and the relative amount of its benzene drops to 25%, corresponding CO 2The content increase is about 200ppm, and its catalytic activity improves, but effect is not clearly.But the one dimension metatitanic acid nanometer band that Mo mixes is greatly improved with respect to its photocatalytic activity of one dimension metatitanic acid nanometer band, and the catalytic activity of the one dimension metatitanic acid nanometer band of Mo+C codope is better than the one dimension metatitanic acid nanometer band that Mo mixes, so the Mo+C codope is for improving its photocatalytic effect have greatly improved (promptly having significant photocatalysis enhancement effect).
Embodiment 2:
The Mo+C codope preparation method of one dimension metatitanic acid nanometer band photocatalyst material, it comprises the steps:
(1) the 45mL butyl titanate is dissolved in the absolute ethyl alcohol of 180mL, adds the glacial acetic acid of 4.5mL then, regulate pH to 3.0, stir with red fuming nitric acid (RFNA) (commercially available);
(2) mass ratio 0.1 of pressing Mo element/Ti element adds ammonium molybdate aqueous solution, stirs 1h, and ultrasonic then dispersions 1.5h 80 ℃ of oven dry down, calcines 3h with the product that obtains down at 500 ℃, obtains mixing the TiO of Mo 2Powder;
(3) will mix the TiO of Mo 2It is that 100mL, concentration are vigorous stirring 30h in the sodium hydroxide solution of 2M that powder 3.33g and 0.1g glucose dissolve in volume, obtains suspension solution;
(4) adopt hydrothermal method hydro-thermal reaction 2 days under 160 ℃ temperature then, adjust pH value to 7.0 by dripping HCl solution (0.1M);
(5) mistake is dried 24h down at 80 ℃ after filtering out filtrate, can obtain the one dimension metatitanic acid (H of Mo+C codope 2Ti 5O 113H 2O) nanometer band photocatalyst material.
The photocatalytic effect of present embodiment is identical with embodiment 1, promptly has greatly improved.
Embodiment 3:
The Mo+C codope preparation method of one dimension metatitanic acid nanometer band photocatalyst material, it comprises the steps:
(1) the 45mL butyl titanate is dissolved in the absolute ethyl alcohol of 180mL, adds the glacial acetic acid of 4.5mL then, regulate pH to 3.0, stir with red fuming nitric acid (RFNA) (commercially available);
(2) mass ratio 6% of pressing Mo element/Ti element adds ammonium molybdate aqueous solution, stirs 1h, and ultrasonic then dispersions 1.5h 80 ℃ of oven dry down, calcines 3h with the product that obtains down at 500 ℃, obtains mixing the TiO of Mo 2Powder;
(3) will mix the TiO of Mo 2It is that 100mL, concentration are vigorous stirring 50h in the sodium hydroxide solution of 20M that powder 3.33g and 1.5g glucose dissolve in volume, obtains suspension solution;
(4) adopt hydrothermal method hydro-thermal reaction 4 days under 220 ℃ temperature then, adjust pH value to 7.0 by dripping HCl solution (0.1M);
(5) mistake is dried 24h down at 80 ℃ after filtering out filtrate, can obtain the one dimension metatitanic acid (H of Mo+C codope 2Ti 5O 113H 2O) nanometer band photocatalyst material.
The photocatalytic effect of present embodiment is identical with embodiment 1, promptly has greatly improved.
Each raw material that the present invention is cited, and the bound of each raw material of the present invention, interval value, and the bound of technological parameter (as temperature, time etc.), interval value can both realize the present invention, do not enumerate embodiment one by one at this.

Claims (2)

1. the Mo+C codope preparation method of one dimension metatitanic acid nanometer band photocatalyst material is characterized in that it comprises the steps:
(1) press butyl titanate: absolute ethyl alcohol: glacial acetic acid=45mL: 180mL: 4.5mL, butyl titanate is dissolved in the absolute ethyl alcohol, add glacial acetic acid then, regulate pH to 3.0 with red fuming nitric acid (RFNA), stir;
(2) mass ratio 0.1～6% of pressing Mo element/Ti element adds ammonium molybdate aqueous solution, stirs 1h, and ultrasonic then dispersions 1.5h 80 ℃ of oven dry down, calcines 3h with the product that obtains down at 500 ℃, obtains mixing the TiO of Mo 2Powder;
(3) by the TiO that mixes Mo 2Powder: glucose: sodium hydroxide solution=3.33g: 0.1～1.5g: 100mL, wherein the concentration of sodium hydroxide solution is 2～20M, chooses the TiO that mixes Mo 2Powder, glucose and sodium hydroxide solution; To mix the TiO of Mo 2Powder and glucose dissolve in the sodium hydroxide solution, stir 30～50h, obtain suspension solution;
(4) then, suspension solution adopts hydrothermal method hydro-thermal reaction 2～4 days under 160～220 ℃ temperature, adjusts pH value to 7.0 by dripping HCl solution;
(5) filter the back and dry 24h down, obtain one dimension metatitanic acid nanometer band photocatalyst material at 80 ℃.
2. the Mo+C codope preparation method of one dimension metatitanic acid nanometer band photocatalyst material according to claim 1, the concentration that it is characterized in that described HCl solution is 0.1M.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103394376A (en) * 2013-07-01 2013-11-20 复旦大学 Method for preparing molybdenum and carbon co-doped titanium dioxide photocatalysis film
CN105344350A (en) * 2015-12-03 2016-02-24 江南大学 Preparation method for molybdenum-doped TiO2 nanowire/graphene compound with high catalytic degradation activity under visible light
CN111097400A (en) * 2019-12-30 2020-05-05 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of C-doped titanium dioxide nanobelt

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CN101643240A (en) * 2008-11-25 2010-02-10 中国科学院合肥物质科学研究院 Method for preparing nanometer titanate with controllable appearances by utilizing industrial raw materials

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CN101643240A (en) * 2008-11-25 2010-02-10 中国科学院合肥物质科学研究院 Method for preparing nanometer titanate with controllable appearances by utilizing industrial raw materials

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103394376A (en) * 2013-07-01 2013-11-20 复旦大学 Method for preparing molybdenum and carbon co-doped titanium dioxide photocatalysis film
CN103394376B (en) * 2013-07-01 2015-04-22 复旦大学 Method for preparing molybdenum and carbon co-doped titanium dioxide photocatalysis film
CN105344350A (en) * 2015-12-03 2016-02-24 江南大学 Preparation method for molybdenum-doped TiO2 nanowire/graphene compound with high catalytic degradation activity under visible light
CN111097400A (en) * 2019-12-30 2020-05-05 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of C-doped titanium dioxide nanobelt

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